Phosphorus sulfide (P2S5) → 2-(2-Chloroethyl)-2,3-dihydro-4-methylnaphth[2,1-f][1,4]oxazepine-5(4H)-thione

HRID 4809

Reaktionsgleichung

Reaktionsgleichung von HRID 4809
P12(SP3(SP(SP(S3)(S1)=S)(=S)S2)=S)=S.[S-2:15].[K+].[K+].[Cl:18][CH2:19][CH2:20][CH:21]1[CH2:27][N:26]([CH3:28])[C:25](=O)[C:24]2[CH:30]=[CH:31][C:32]3[C:37]([C:23]=2[O:22]1)=[CH:36][CH:35]=[CH:34][CH:33]=3>C1(C)C=CC=CC=1>[Cl:18][CH2:19][CH2:20][CH:21]1[CH2:27][N:26]([CH3:28])[C:25](=[S:15])[C:24]2[CH:30]=[CH:31][C:32]3[C:37]([C:23]=2[O:22]1)=[CH:36][CH:35]=[CH:34][CH:33]=3

Komponenten

5

Edukt 3

HCID 14817Phosphorus sulfide (P2S5)HCID 162263Potassium SulfideHCID 137263702-(2-chloroethyl)-2,3-dihydro-4-methylnaphth[2,1-f][1,4]oxazepin-5(4H)-one

Produkt 1

HCID 137263712-(2-Chloroethyl)-2,3-dihydro-4-methylnaphth[2,1-f][1,4]oxazepine-5(4H)-thioneAusbeute 84,1 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 1140TolueneLösungsmittel

Versuchsvorschrift

A mixture of 9.55 g of phosphorus pentasulfide and 9.5 g of potassium sulfide were ground together and added to a solution of 20.2 g (0.07 mole) of 2-(2-chloroethyl)-2,3-dihydro-4-methylnaphth[2,1-f][1,4]oxazepin-5(4H)-one in 200 ml of dry toluene. The mixture was stirred and heated at reflux for 7 hr. The hot reaction mixture was filtered and the product crystallized from the cooled filtrate. Recrystallization from chloroform gave 18 g (84%) of yellow crystals, m.p. 167°-170° C.

Aufarbeitung

  1. temperatureheated
  2. temperatureat reflux for 7 hr
  3. filtrationThe hot reaction mixture was filtered
  4. customthe product crystallized from the cooled filtrate
  5. customRecrystallization from chloroform

Quellen und Nachweise

ORD-Eintrag
ord-dbc1d0fc06cc4d08ac04f8d8f4685b9b
Quelldatensatz
uspto-grants-1988_02
Patentnummer
US04727152

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